CN110165143A - A kind of lithium battery electrode plate and the preparation method and application thereof - Google Patents

A kind of lithium battery electrode plate and the preparation method and application thereof Download PDF

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Publication number
CN110165143A
CN110165143A CN201910439676.3A CN201910439676A CN110165143A CN 110165143 A CN110165143 A CN 110165143A CN 201910439676 A CN201910439676 A CN 201910439676A CN 110165143 A CN110165143 A CN 110165143A
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binder
preparation
active material
covering
electrode slice
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单洁
母飞
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DONGGUAN ADF BATTERY Co Ltd
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DONGGUAN ADF BATTERY Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/661—Metal or alloys, e.g. alloy coatings
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a kind of lithium battery electrode plates and the preparation method and application thereof.The present invention is sintered after the active material containing binder and covering is coated in collector, binder and covering therein are sintered carbonization, on the one hand, binder and covering after carbonization are coated on active material surface, core-shell structure is formed, on the other hand, active material and collector can be bonded together by remaining hydrogen bond and Van der Waals force well after binder carbonization, the binder is carbonized rear electric conductivity enhancing simultaneously, plays the role of " killing two birds with one stone ".In addition, the present invention improves the preparation method of electrode slice from " source ", to fundamentally improve the electric conductivity of electrode, compared to being coated, adulterated or mixed conductivity substance has simpler more stable advantage to active material, this method is also easy to realize, original preparation process and equipment are changed without excessive, are conducive to be mass produced.

Description

A kind of lithium battery electrode plate and the preparation method and application thereof
Technical field
The present invention relates to field of lithium more particularly to a kind of lithium battery electrode plate and the preparation method and application thereof.
Background technique
Spinel lithium titanate has lithium ion deintercalation structure zero strain as lithium battery material of new generation, and embedding lithium point is high (1.5V vs Li/Li+), it can be used as anode and negative electrode material use.And voltage platform is steady, and cyclicity is excellent, security performance The features such as high is a kind of very promising lithium battery material.But the electron conduction of lithium titanate is poor, so that it is in charge and discharge High rate performance in the process is poor, and common improved method is doped chemical during synthesizing lithium titanate, controls crystallite dimension, packet Cover conductive material etc..Meanwhile microelectronic component type and quantity are more and more, and the battery small for large scale preparation mentions Higher requirement is gone out.
All contain binder in the electrode slice of existing lithium battery, the presence of binder weakens electrode to a certain extent The electric conductivity of material, especially for being even more to make the matter worse for the poor active material of electric conductivity itself, but if not making With binder, active material can not be bonded in copper foil or aluminum foil current collector, because copper foil and aluminium foil surface are very smooth, nothing Method attachment activity material.
Therefore, in order to further increase the electric conductivity of electrode slice, especially for the activity that electric conductivity itself is poor Material, it is necessary to the preparation method of original electrode slice be improved, and further increase the performance of battery from " source ", had There is prior practical significance.
Summary of the invention
The purpose of the present invention is to provide a kind of lithium battery electrode plate and the preparation method and application thereof, the present invention will be containing viscous The active material of knot agent and covering is sintered after being coated in collector, and binder and covering therein are sintered carbon Change, on the one hand, binder and covering after carbonization are coated on active material surface, form core-shell structure, on the other hand, bonding Active material and collector can be bonded together by remaining hydrogen bond and Van der Waals force well after agent carbonization, thus by active Material adheres on a current collector, at the same the binder be carbonized after also further enhance the electric conductivity of electrode slice.
Technical solution of the present invention is specific as follows:
One of the objects of the present invention is to provide a kind of lithium battery electrode plate, the electrode slice is living comprising collector, carbon coating Property material, wherein the carbon coating active material is core-shell structure, and binder, the collector are not contained in the electrode slice Any one in copper foil, aluminium foil.
Preferably, the ratio of the quality Yu active material quality of carbon-coating is 1:(20 in carbon coating active material described above ~200)；More preferably 1:100.
Preferably, above-mentioned collector with a thickness of 6~15 μm.
Preferably, above-mentioned active material be selected from lithium titanate, cobalt acid lithium, LiMn2O4, nickel ion doped, nickel-cobalt-manganese ternary material, At least one of lithium-rich manganese base material.
Above-mentioned electrode slice is positive plate or negative electrode tab.
Another object of the present invention is to provide the preparation methods of above-mentioned electrode slice, include the following steps:
1) covering, binder and solvent are mixed, obtains sol solution；
2) active material is added in sol solution, obtains slurry；
3) slurry is coated on collector, drying, rear starvation sintering, after covering and binder sintering carbonization Electrode slice.
Preferably, the mass ratio of the covering in step 1), binder and solvent is (2~8): 1:(30~85).
Preferably, above-mentioned covering is selected from least one of polyethylene glycol oxide, hydrolytic lignin, acetic acid lignin.
Preferably, above-mentioned binder is selected from Kynoar.
Preferably, the relative molecular weight of above-mentioned binder is 2000~3000；More preferably 2000~2200.
Preferably, above-mentioned solvent is selected from least one of dimethylformamide, N-Methyl pyrrolidone.
Preferably, the mixing temperature in step 1) is 40~80 DEG C.
Preferably, further include the steps that being stirred during mixing in step 1), it is preferable that mixing time 0.1 ~5h；More preferably 0.5~3h.
Preferably, the mass ratio of binder is (50~90) in the active material and sol solution in step 2): 1；More preferably For (65~80): 1.
Preferably, the granularity of the active material in step 2) is 5~15 μm, more preferably: 8~12 μm.
Preferably, in step 3) by slurry be coated on collector on a thickness of 5~200 μm；More preferably 80~150 μ m。
Preferably, the slurry in step 3) is the slurry after sieving with 100 mesh sieve.
Preferably, the sintering temperature in step 3) is 500~700 DEG C；More preferably 550~650 DEG C.
Preferably, the sintering time in step 3) is 0.5~5h；More preferably 2~4h.
Preferably, the heating rate in step 3) is 0.5~10 DEG C/min.
It include above-mentioned electrode slice in the lithium battery the present invention also provides a kind of lithium battery.
Preferably, above-mentioned lithium battery is miniature lithium battery；Preferably, which uses aluminum plastic film for shell progress Encapsulation, inside be made of the positive plate, diaphragm, negative electrode tab of successively lamination, electrolyte permeability wherein, positive plate or cathode therein Piece is above-mentioned electrode slice.
The beneficial effects of the present invention are:
1, invention is sintered after the active material containing binder and covering is coated in collector, therein Binder and covering are sintered carbonization, on the one hand, binder and covering after carbonization are coated on active material surface, are formed Core-shell structure, on the other hand, remaining hydrogen bond and Van der Waals force can be well by active materials and afflux after binder carbonization Body is bonded together, while the binder is carbonized rear electric conductivity enhancing, plays the role of " killing two birds with one stone ".
2, the present invention improves the preparation method of electrode slice from " source ", to fundamentally improve the conduction of electrode Property, compared to being coated, adulterated or mixed conductivity substance has simpler more stable advantage, the party to active material Method is also easy to realize, original preparation process and equipment is changed without excessive, are conducive to be mass produced.
Specific embodiment
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art are according to the present invention Some nonessential modifications and adaptations that the principle of elaboration is made all belong to the scope of protection of the present invention.Following specific works of example Skill parameter etc. is also only an example in OK range, i.e. those skilled in the art can do suitable model by the explanation of this paper Interior selection is enclosed, and does not really want to be defined in hereafter exemplary specific data.
Embodiment 1
A kind of preparation method of lithium battery electrode plate, includes the following steps:
1) 2 parts of polyethylene glycol oxides, 1 part of Kynoar (PVDF), 30 parts of N-Methyl pyrrolidones are weighed, are stirred in 40 DEG C 0.5h obtains sol solution；
2) lithium titanate that 50 parts of granularities are 5 μm is added in sol solution, persistently stirs 1h, is uniformly mixed, obtains slurry；
3) coated in 8 μm of copper foil current collector after sieving with 100 mesh sieve slurry, coating thickness is 5 μm, is dried in 50 DEG C of air blast Case is dry for 24 hours, after be put into tube furnace, 500 DEG C of sintering are warming up to the heating rate of 5 DEG C/min in argon atmosphere and are carbonized 2h obtains electrode slice after cooling.
Embodiment 2
A kind of preparation method of lithium battery electrode plate, includes the following steps:
1) 2 parts of hydrolytic lignins, 1 part of PVDF, 50 parts of N-Methyl pyrrolidones are weighed, in 50 DEG C of stirring 3h, obtain sol solution；
2) lithium titanate that 60 parts of granularities are 5 μm is added in sol solution, persistently stirs 1h, is uniformly mixed, obtains slurry；
3) it is coated in 6 μm of copper foil current collectors after sieving with 100 mesh sieve slurry, coating thickness is 5 μm, in 50 DEG C of convection ovens It is dry for 24 hours, after be put into tube furnace, 500 DEG C of sintering are warming up to the heating rate of 5 DEG C/min in nitrogen atmosphere and are carbonized 2h, Electrode slice is obtained after cooling.
Embodiment 3
A kind of preparation method of lithium battery electrode plate, includes the following steps:
1) 8 parts of hydrolytic lignins, 1 part of PVDF, 85 parts of N-Methyl pyrrolidones are weighed, in 80 DEG C of stirring 3h, obtain sol solution；
2) lithium titanate that 90 parts of granularities are 15 μm is added in sol solution, persistently stirs 1h, is uniformly mixed, obtains slurry；
3) it is coated in 8 μm of copper foil current collectors after sieving with 100 mesh sieve slurry, coating thickness is 5 μm, in 50 DEG C of convection ovens It is dry for 24 hours, after be put into tube furnace, 700 DEG C of sintering are warming up to the heating rate of 5 DEG C/min in argon atmosphere and are carbonized 2h, Electrode slice is obtained after cooling.
Embodiment 4
A kind of preparation method of lithium battery electrode plate, includes the following steps:
1) 6 parts of hydrolytic lignins, 1 part of PVDF, 50 parts of N-Methyl pyrrolidones are weighed, in 50 DEG C of stirring 3h, obtain sol solution；
2) lithium titanate that 80 parts of granularities are 8 μm is added in sol solution, persistently stirs 1h, is uniformly mixed, obtains slurry；
3) it is coated in 12 μm of copper foil current collectors after sieving with 100 mesh sieve slurry, coating thickness is 5 μm, is dried in 80 DEG C of air blast Case is dry for 24 hours, after be put into tube furnace, 600 DEG C of sintering are warming up to the heating rate of 5 DEG C/min in nitrogen atmosphere and are carbonized 2h obtains electrode slice after cooling.
Embodiment 5
A kind of preparation method of lithium battery electrode plate, includes the following steps:
1) 4 parts of acetic acid lignins, 1 part of PVDF, 65 parts of dimethylformamides are weighed, in 50 DEG C of stirring 3h, obtain sol solution；
2) lithium titanate that 60 parts of granularities are 5 μm is added in sol solution, persistently stirs 1h, is uniformly mixed, obtains slurry；
3) it is coated in 12 μm of copper foil current collectors after sieving with 100 mesh sieve slurry, coating thickness is 5 μm, is dried in 50 DEG C of air blast Case is dry for 24 hours, after be put into tube furnace, 500 DEG C of sintering are warming up to the heating rate of 5 DEG C/min in argon atmosphere and are carbonized 4h obtains electrode slice after cooling.
Embodiment 6
A kind of preparation method of lithium battery electrode plate, includes the following steps:
1) 3 parts of acetic acid lignins, 1 part of PVDF, 75 parts of N-Methyl pyrrolidones are weighed, in 50 DEG C of stirring 3h, obtain sol solution；
2) lithium titanate that 75 parts of granularities are 10 μm is added in sol solution, persistently stirs 1h, is uniformly mixed, obtains slurry；
3) it is coated in 8 μm of copper foil current collectors after sieving with 100 mesh sieve slurry, coating thickness is 200 μm, is dried in 60 DEG C of air blast Case is dry for 24 hours, after be put into tube furnace, 600 DEG C of sintering are warming up to the heating rate of 5 DEG C/min in argon atmosphere and are carbonized 2h obtains electrode slice after cooling.
Embodiment 7
A kind of preparation method of lithium battery electrode plate, includes the following steps:
1) 2 parts of hydrolytic lignins, 1 part of PVDF, 50 parts of N-Methyl pyrrolidones are weighed, in 50 DEG C of stirring 3h, obtain sol solution；
2) lithium titanate that 80 parts of granularities are 12 μm is added in sol solution, persistently stirs 1h, is uniformly mixed, obtains slurry；
3) it is coated in 15 μm of copper foil current collectors after sieving with 100 mesh sieve slurry, coating thickness is 100 μm, in 60 DEG C of air blast Oven drying for 24 hours, after be put into tube furnace, 600 DEG C of sintering carbonization is warming up to the heating rate of 5 DEG C/min in nitrogen atmosphere 4h obtains electrode slice after cooling.
Embodiment 8
A kind of preparation method of lithium battery electrode plate, includes the following steps:
1) 4 parts of polyethylene glycol oxides, 1 part of PVDF, 65 parts of N-Methyl pyrrolidones are weighed, in 50 DEG C of stirring 3h, obtain sol solution；
2) lithium titanate that 85 parts of granularities are 8 μm is added in sol solution, persistently stirs 1h, is uniformly mixed, obtains slurry；
3) it is coated in 6 μm of copper foil current collectors after sieving with 100 mesh sieve slurry, coating thickness is 120 μm, is dried in 50 DEG C of air blast Case is dry for 24 hours, after be put into tube furnace, 700 DEG C of sintering are warming up to the heating rate of 5 DEG C/min in argon atmosphere and are carbonized 2h obtains electrode slice after cooling.
Embodiment 9
A kind of preparation method of lithium battery electrode plate, includes the following steps:
1) 2 parts of polyethylene glycol oxides, 1 part of PVDF, 85 parts of N-Methyl pyrrolidones are weighed, in 60 DEG C of stirring 2h, obtain sol solution；
2) lithium titanate that 50 parts of granularities are 15 μm is added in sol solution, persistently stirs 1h, is uniformly mixed, obtains slurry；
3) it is coated in 8 μm of copper foil current collectors after sieving with 100 mesh sieve slurry, coating thickness is 150 μm, is dried in 80 DEG C of air blast Case is dry for 24 hours, after be put into tube furnace, 500 DEG C of sintering are warming up to the heating rate of 5 DEG C/min in argon atmosphere and are carbonized 2h obtains electrode slice after cooling.
Comparative example 1
A kind of preparation method of lithium battery electrode plate, includes the following steps:
1) 2 parts of conductive agent SP, 1 part of PVDF, 30 parts of N-Methyl pyrrolidones are weighed, in 40 DEG C of stirring 0.5h, obtain sol solution；
2) lithium titanate that 50 parts of granularities are 5 μm is added in sol solution, persistently stirs 1h, is uniformly mixed, obtains slurry；
3) it is coated in 8 μm of copper foil current collectors after sieving with 100 mesh sieve slurry, coating thickness is 5 μm, in 50 DEG C of convection ovens Drying for 24 hours, obtains electrode slice.
Performance test:
Electrode slice prepared by Examples 1 to 9 and comparative example 1 is cut into the specification of 2cm*2cm, with the gold of 2.1cm*2.1cm Belong to lithium piece as cathode, diaphragm uses 16 μm of single spreading diaphragms of Ube, and electrolyte is to contain 1mol/L LiPF6Electrolysis Matter, solvent EC+DEC+DMC, wherein the volume ratio of EC, DEC and MC are 1:1:1 (Xin Zhou nation), rear to use the 113 of Showa electrician μm aluminum plastic film, which successively folds electrode slice, diaphragm, lithium piece in drying shed, to be put into plastic-aluminum putamina, is injected electrolyte, is then used Sealing machine is packaged into minicell.
The minicell of above-mentioned preparation is carried out in the Neware battery test system that Shenzhen Xin Wei Co., Ltd produces Test, test voltage range are 1.0~2.5V, and first charge-discharge multiplying power is 0.1C, and the second circle carries out charge-discharge test using 1C, As a result it see the table below 1:
Table 1
As shown in Table 1: electrode slice prepared by the present invention has extraordinary cycle performance, improves relative to comparative example 1 About 6.5~12.5%, and embedding lithium, de- lithium capacity and first effect have different degrees of raising, while electrode slice of the invention is not It is additional that conductive agent is added, and additional conductive agent is added in comparative example 1, this illustrates that preparation method of the invention can be mentioned further In addition the electric conductivity of high electrode piece also illustrates that this method has certain feasibility, establish for later further development Basis.

Claims (10)

1. a kind of lithium battery electrode plate, it is characterised in that: the electrode slice includes collector, carbon coating active material, wherein institute Stating carbon coating active material is core-shell structure, does not contain binder in the electrode slice；The collector is in copper foil, aluminium foil Any one.
2. electrode slice according to claim 1, it is characterised in that: the quality and work of carbon-coating in the carbon coating active material Property quality of materials ratio be 1:20~200.
3. electrode slice according to claim 1 or 2, it is characterised in that: the active material be selected from lithium titanate, cobalt acid lithium, At least one of LiMn2O4, nickel ion doped, nickel-cobalt-manganese ternary material, lithium-rich manganese base material.
4. the preparation method of electrode slice described in claims 1 to 3 any one, characterized by the following steps:
1) covering, binder and solvent are mixed, obtains sol solution；
2) active material is added in sol solution, mixes, obtains slurry；
3) by slurry coated on collector, drying, rear starvation sintering obtains electrode after covering and binder sintering carbonization Piece.
5. the preparation method according to claim 4, it is characterised in that: covering described in step 1), binder and solvent Mass ratio be 2~8:1:30~85；Preferably, it is wooden to be selected from polyethylene glycol oxide, hydrolytic lignin, acetic acid for the covering At least one of element；Preferably, the binder is selected from Kynoar；Preferably, the solvent is selected from dimethyl formyl At least one of amine, N-Methyl pyrrolidone.
6. the preparation method according to claim 4, it is characterised in that: the mixing temperature in step 1) is 40~80 DEG C.
7. the preparation method according to claim 4, it is characterised in that: glued in active material described in step 2) and sol solution The mass ratio for tying agent is 50~90:1.
8. the preparation method according to claim 4, it is characterised in that: slurry is coated on the thickness on collector in step 3) Degree is 5~200 μm.
9. the preparation method according to claim 4, it is characterised in that: the sintering temperature in step 3) is 500~700 DEG C； Preferably, the sintering time in step 3) is 0.5~5h.
10. a kind of lithium battery, it is characterised in that: include electrode described in claims 1 to 3 any one in the lithium battery Piece.
CN201910439676.3A 2019-05-24 2019-05-24 A kind of lithium battery electrode plate and the preparation method and application thereof Pending CN110165143A (en)

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WO2023168585A1 (en) * 2022-03-08 2023-09-14 宁德新能源科技有限公司 Electrochemical apparatus and electronic device

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Application publication date: 20190823